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In situ X-ray analysis of mesophase formation in random copolymers of propylene and 1-butene

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Abstract

The solidification of random isotactic copolymers of propylene and 1-butene has been followed in real time by wide-angle X-ray scattering as a function of the rate of cooling the quiescent liquid. The experimental setup allowed simultaneous recording of cooling curves—sample temperature as a function of time—and X-ray patterns at high sampling rate of 20 Hz. This approach allowed establishing a correlation between cooling rate, temperature of crystallization/mesophase formation, and X-ray structure, which formerly has only been observed ex situ, after completion of structure formation during cooling and subsequent aging. It is quantitatively confirmed that addition of 1-butene co-units into the propylene chain allows mesophase formation on cooling the melt at distinctly lower rate than in case of the homopolymer. The experimental results are compiled into a continuous cooling transformation (CCT) diagram and compared with data obtained earlier on random copolymers of propylene with ethylene.

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Acknowledgments

Financial support by the Deutsche Forschungsgemeinschaft (DFG) for two of the authors (DM, RA) and by ESRF is gratefully acknowledged. Furthermore, we thank the team of the beamline BM26B/Dubble at ESRF for their assistance in temperature-resolved X-ray measurements.

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Authors and Affiliations

  1. Center of Engineering Sciences, Martin-Luther-University Halle-Wittenberg, 06099, Halle/Saale, Germany

    Daniela Mileva & René Androsch

  2. Department of Chemistry and Industrial Chemistry, University of Genova, via Dodecaneso 31, 16146, Genoa, Italy

    Dario Cavallo, Lorenza Gardella & Giovanni C. Alfonso

  3. ESRF, Dubble CRG, Netherlands Organization of Scientific Research (NWO), 38043, Grenoble, France

    Giuseppe Portale

  4. Department of Mechanical Engineering, Eindhoven University of Technology, P.O. Box 513, 5600 MB, Eindhoven, The Netherlands

    Luigi Balzano

Authors
  1. Daniela Mileva
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  2. Dario Cavallo
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  3. Lorenza Gardella
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  4. Giovanni C. Alfonso
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  5. Giuseppe Portale
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  6. Luigi Balzano
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  7. René Androsch
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Correspondence to René Androsch.

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Mileva, D., Cavallo, D., Gardella, L. et al. In situ X-ray analysis of mesophase formation in random copolymers of propylene and 1-butene. Polym. Bull. 67, 497–510 (2011). https://doi.org/10.1007/s00289-011-0487-y

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  • DOI: https://doi.org/10.1007/s00289-011-0487-y

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